WO2017086084A1 - Procédé de réparation pour membrane de séparation et procédé de fabrication de structure de membrane de séparation - Google Patents

Procédé de réparation pour membrane de séparation et procédé de fabrication de structure de membrane de séparation Download PDF

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Publication number
WO2017086084A1
WO2017086084A1 PCT/JP2016/081077 JP2016081077W WO2017086084A1 WO 2017086084 A1 WO2017086084 A1 WO 2017086084A1 JP 2016081077 W JP2016081077 W JP 2016081077W WO 2017086084 A1 WO2017086084 A1 WO 2017086084A1
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WIPO (PCT)
Prior art keywords
separation membrane
support
repair material
repair
material particles
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PCT/JP2016/081077
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English (en)
Japanese (ja)
Inventor
慎一郎 山崎
健史 萩尾
憲一 野田
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日本碍子株式会社
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Application filed by 日本碍子株式会社 filed Critical 日本碍子株式会社
Priority to CN201680056179.XA priority Critical patent/CN108290123B/zh
Priority to JP2017551785A priority patent/JP6767995B2/ja
Priority to DE112016005301.0T priority patent/DE112016005301T5/de
Publication of WO2017086084A1 publication Critical patent/WO2017086084A1/fr
Priority to US15/972,687 priority patent/US11471836B2/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
    • B01D65/106—Repairing membrane apparatus or modules
    • B01D65/108—Repairing membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B01D69/108—Inorganic support material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/028—Molecular sieves
    • B01D71/0281—Zeolites

Definitions

  • the present invention relates to a method for repairing a separation membrane and a method for manufacturing a separation membrane structure.
  • the present invention has been made in view of the above situation, and an object thereof is to provide a separation membrane repair method and a separation membrane structure manufacturing method capable of improving the separation performance of the separation membrane.
  • the method for repairing a separation membrane according to the present invention includes a step of attaching a colloidal solution having a predetermined pH in which repair material particles are dispersed in an aqueous solvent to the surface of the separation membrane formed on a support. At a predetermined pH, the repair material particles have a charge opposite to that of the support.
  • FIG. 1 is a cross-sectional view showing the configuration of the separation membrane structure 10.
  • the separation membrane structure 10 includes a support 20, a separation membrane 30, and a repair unit 40.
  • the support 20 supports the separation membrane 30.
  • the support 20 has chemical stability such that the separation membrane 30 can be formed into a film shape (crystallization, coating, or deposition) on the surface.
  • the support 20 is a ceramic sintered body. Examples of the ceramic include alumina, silica, mullite, zirconia, titania, yttria, silicon nitride, and silicon carbide.
  • the support 20 may have any shape that can supply the fluid mixture to be separated to the separation membrane 30.
  • Examples of the shape of the support 20 include a monolith shape, a flat plate shape, a tubular shape, a cylindrical shape, a columnar shape, and a prismatic shape.
  • the monolith shape is a shape having a plurality of cells formed in the longitudinal direction, and is a concept including a honeycomb shape.
  • the length in the longitudinal direction can be 150 to 2000 mm
  • the diameter in the radial direction can be 30 to 220 mm, but is not limited thereto.
  • 30 to 2500 cells having a diameter of 1 to 5 mm can be formed on the support 20.
  • the support 20 is a porous body having a large number of open pores.
  • the average pore diameter of the support 20 may be a size that allows a permeated component that has permeated through the separation membrane 30 in the fluid mixture to pass therethrough.
  • the porosity of the support 20 is not particularly limited, but may be, for example, 25% to 50%.
  • the average pore diameter of the support 20 is not particularly limited, but can be, for example, 0.01 ⁇ m or more and 25 ⁇ m or less.
  • the average pore diameter of the support 20 can be measured with a mercury porosimeter or a palm porometer.
  • the average particle size of the support 20 is not particularly limited, but may be, for example, 5 ⁇ m or more and 100 ⁇ m or less.
  • the average particle diameter of the support 20 is an arithmetic average value of the maximum diameter of each of the 30 particles measured by cross-sectional observation using SEM (Scanning Electron Microscope).
  • the support 20 may be composed of a single layer having a uniform average pore diameter, or may be composed of a plurality of layers each having a different average pore diameter. When the support 20 is composed of multiple layers, the average pore diameter of each layer may be smaller as it is closer to the separation membrane 30. When the support 20 is composed of multiple layers, the average pore diameter of the support 20 means the average pore diameter of the layer in contact with the separation membrane 30. In the case where the support 20 is composed of multiple layers, each layer can be composed of at least one material selected from the materials described above.
  • the separation membrane 30 is formed on the support 20.
  • the separation membrane 30 can be composed of an inorganic material, an organic material, a metal material, or a composite material thereof. Considering heat resistance and organic solvent resistance, the separation membrane 30 is preferably an inorganic membrane such as a zeolite membrane, titania membrane, silica membrane, or carbon membrane, and more preferably a zeolite membrane that tends to narrow the pore size distribution. It is.
  • the average pore diameter of the separation membrane 30 is smaller than the average pore diameter of the support 20.
  • the average pore diameter of the separation membrane 30 can be 0.001 to 1.0 ⁇ m.
  • the average pore size of the separation membrane 30 is determined by the air flow method or mercury intrusion method described in ASTM F316 (Standard Test Methods for Pore Size Characteristics of Membrane Filters by Bubble Point and Mean Flow Pore Test). It can be measured.
  • the separation membrane 30 is a zeolite membrane having pores composed of rings having an oxygen n-membered ring or less
  • the average pore diameter of the separation membrane 30 is an arithmetic average value of the short diameter and long diameter of the pores.
  • the oxygen n-membered ring means that the number of oxygen atoms constituting the skeleton forming the pore is n and includes at least one of Si atom, Al atom and P atom, and each oxygen atom is Si atom. It is a part that forms a cyclic structure by bonding with Al atom or P atom.
  • the framework structure (type) of the zeolite is not particularly limited.
  • AEI, CHA, DDR, AFX, MFI, FAU, MOR, BEA, LTA and RHO are preferred because the zeo
  • the separation membrane 30 includes a plurality of defects 31.
  • the defect 31 penetrates the separation membrane 30 in the thickness direction.
  • the defect 31 continues to the outer surface 30S of the separation membrane 30 and the interface 30T between the separation membrane 30 and the support 20.
  • the number of defects 31 is not particularly limited.
  • the average inner diameter of the defect 31 is not particularly limited, but can be, for example, 5 nm or more and 10 ⁇ m or less.
  • the average inner diameter of the defect 31 is an arithmetic average value of the maximum diameters of the respective defects 31 in the plane direction orthogonal to the thickness direction.
  • the repair unit 40 is disposed inside the defect 31. It is preferable that the repair part 40 is filled in the defect 31. When the repair unit 40 closes the defect 31, it is possible to suppress components other than the permeation component contained in the fluid mixture from passing through the defect 31.
  • the repair part 40 is an aggregate of ceramics.
  • the ceramic include silica, titania, alumina, mullite, zirconia, yttria, silicon nitride, silicon carbide, and the like, and silica, titania, alumina, and zirconia are preferable in view of handling and availability.
  • the average particle diameter of the ceramic particles constituting the repaired part 40 is not particularly limited, but can be 2 nm or more and 5 ⁇ m or less. It is preferable that the average particle diameter of the ceramic particles constituting the repaired portion 40 is smaller than the average inner diameter of the defect 31.
  • the average particle diameter of the ceramic particles is an arithmetic average value of the maximum diameters of each of the 30 particles measured by observation using SEM (Scanning Electron Microscope) or TEM (Transmission Electron Microscope).
  • a molded body of the support 20 is formed by forming the raw material of the support 20 into a desired shape using an extrusion molding method, a press molding method, a cast molding method, or the like. .
  • the molded body of the support 20 is fired (for example, 900 ° C. to 1450 ° C.) to form the support 20.
  • the separation membrane 30 is formed on the support 20.
  • a method for forming a zeolite membrane and a titania membrane as an example of the separation membrane 30 will be described in order.
  • zeolite as a seed crystal is coated on the surface of the support 20 in advance, and then the support 20 is placed in a pressure vessel containing a raw material solution containing a silica source, an alumina source, an organic template, an alkali source, water, and the like. Immerse.
  • the pressure-resistant container is placed in a dryer and subjected to heat treatment (hydrothermal synthesis) at 100 to 200 ° C. for 1 to 240 hours to form a zeolite membrane.
  • the support 20 on which the zeolite membrane is formed is washed and dried at 80 to 100 ° C.
  • the support 20 is put in an electric furnace and heated at 400 to 800 ° C. in the atmosphere for about 1 to 200 hours to burn and remove the organic template. At this time, a plurality of defects 31 are generated in the obtained zeolite membrane.
  • a mixed solution of metal alkoxide (titanium tetraisopropoxide) and nitric acid or hydrochloric acid is mixed with water, and further mixed with alcohol or water previously mixed with nitric acid to obtain a titania sol stock solution.
  • a titania sol coating solution is obtained by diluting the titania sol stock solution with alcohol or water.
  • the excess titania sol coating liquid is removed.
  • a titania film is formed by heating at 400 to 500 ° C. for about 1 to 10 hours. At this time, a plurality of defects 31 are generated in the obtained titania film.
  • a colloid solution is prepared by dispersing repair material particles in an aqueous solvent.
  • the repair material particles include ceramic particles such as silica particles, titania particles, alumina particles, mullite particles, zirconia particles, yttria particles, silicon nitride particles, and silicon carbide particles.
  • the average particle diameter of the repair material particles is not particularly limited, but is preferably 2 nm or more and 5 ⁇ m or less. By setting the average particle diameter of the repair material particles to 2 nm or more, the repair material particles can be prevented from diffusing into the support 20. In addition, by setting the average particle diameter of the repair material particles to 5 ⁇ m or less, the repair material particles can smoothly flow into the defect 31.
  • the concentration of the repair material particles in the colloidal solution is not particularly limited, but is preferably 0.01% by mass or more and 20% by mass or less. By setting the concentration of the repair material particles to 0.01% by mass or more, a sufficient number of repair material particles can flow into the defect 31. In addition, by setting the concentration of the repair material particles to 20% by mass or less, it is possible to suppress the repair material particles from being excessively attached to the surface of the separation membrane 30 and remaining.
  • aqueous solvent means a solvent containing water.
  • concentration of water in the colloidal solution is not particularly limited, but the occupancy ratio of water with respect to the total solvent can be, for example, 50% by mass or more and 100% by mass or less.
  • colloidal solution is adjusted to predetermined pH.
  • the pH of the colloidal solution is determined in consideration of the charge generated according to the zeta potential of the support 20, the separation membrane 30, and the repair material particles.
  • the zeta potential of the support 20, the separation membrane 30, and the repair material particles is a zeta potential that is generated when each comes into contact with the solvent of the colloidal solution.
  • the charges generated in the support 20, the separation membrane 30, and the repair material particles are charges of the respective zeta potentials.
  • the zeta potential generated in each of the repair material particles for forming the support 20, the separation membrane 30, and the repair portion 40 varies, so the colloid solution so that an appropriate charge relationship is established. It is necessary to determine the pH.
  • FIG. 2 is a graph showing the relationship between the pH of the colloidal solution and the zeta potential for the main materials.
  • a first pH range in which the repair material particles have a charge with a sign opposite to that of the support 20 is examined.
  • a second pH range in which the separation membrane 30 has the same sign as that of the repair material particles is examined.
  • a third pH range is examined such that the absolute value of the zeta potential of the separation membrane 30 is equal to or less than the absolute value of the zeta potential of the repair material particles.
  • the predetermined pH of the colloidal solution may be within the first pH range, but is preferably within the second pH range, and more preferably within the third pH range. For materials other than those shown in FIG. 2, the relationship between the pH of a known colloidal solution and the zeta potential can be used.
  • the support 20 is made of alumina
  • the separation membrane 30 is made of titania
  • silica particles are used as repair material particles will be described as an example in the first to third pH ranges.
  • the first pH range in which alumina has a positive charge and silica particles have a negative charge is 3 to 8.5.
  • the second pH range in which titania has the same negative charge as the silica particles is 7 to 8.5.
  • the third pH range in which the absolute value of titania's zeta potential is less than or equal to the absolute value of the zeta potential of silica particles is the second pH range 7 to 8. It overlaps with 5. Therefore, when the support 20 is made of alumina, the separation membrane 30 is made of titania, and silica particles are used as the repair material particles, the colloidal solution can be brought into the first pH range of 3 to 8.5. Although it is good, it is preferable to enter the second and third pH ranges of 7 to 8.5.
  • a colloidal solution adjusted to a predetermined pH is adhered to the surface of the separation membrane 30.
  • the method for attaching the colloidal solution is not particularly limited, a flow-down method or a coating method can be used.
  • the aqueous solvent in the colloidal solution also contacts the support 20 through the defect 31 of the separation membrane 30. Therefore, a zeta potential (see FIG. 2) specific to each constituent material is generated in the support material 20, the separation membrane 30, and the repair material particles in the colloid solution.
  • FIG. 3A illustrates a case where the support 20 has a positive charge, and the separation membrane 30 and the repair material particles have a negative charge. Since the repair material particles have a charge opposite to that of the support 20, the repair material particles are attracted to the support 20 by the Coulomb force and attracted to the defect 31 as shown in FIG. At this time, if the separation membrane 30 has the same charge as the repair material particles, the repair material particles are not attracted to the separation membrane 30 by the Coulomb force, so that the repair material particles can be efficiently put into the defect 31. it can.
  • the repair material particles can be suppressed from repelling the separation membrane 30, so that the repair material particles are more efficient due to the defects 31. Can be put in.
  • the excess colloidal solution adhering to the surface of the separation membrane 30 is removed. Thereby, the repair material particles remaining on the surface of the separation membrane 30 can be reduced, and the reduction of the separation coefficient of the separation membrane 30 can be suppressed.
  • the method for removing the colloidal solution is not particularly limited, and the colloidal solution may be blown off with a blower or the like, or the colloidal solution may be wiped off directly.
  • the colloidal solution that has entered the defect 31 is dried.
  • the aqueous solvent in the colloidal solution evaporates to form the repaired portion 40 that is an aggregate of ceramics.
  • the method for drying the colloidal solution is not particularly limited, and may be naturally dried at room temperature or heat treated at a temperature of 200 ° C. or lower. In the case of natural drying at room temperature, the apparatus and process can be simplified. When the heat treatment is performed at a temperature of 200 ° C. or lower, the colloidal solution can be quickly dried.
  • a clay was prepared by adding water, a dispersant, and a thickener to alumina particles (aggregate) having an average particle size of 50 ⁇ m, and mixing and kneading.
  • a formed body of a honeycomb-shaped columnar support was formed by extruding the obtained clay.
  • the molded body was fired at 900-1500 ° C. to form a support.
  • the outer diameter of the support was 30 mm
  • the length of the support was 160 mm
  • the inner diameter of each of the 30 cells was 2.3 mm.
  • DDR type zeolite crystal powder was produced as a seed crystal. And after disperse
  • the DDR concentration was adjusted to 0.001 to 0.36% by mass by diluting the seed crystal dispersion with ethanol.
  • the slurry liquid for seeding was produced by stirring at 300 rpm using a stirrer.
  • the support was fixed to the lower end of the wide-mouth funnel, and 160 ml of the seeding slurry liquid was poured into each cell from above the support and passed therethrough. Thereafter, each cell was air-dried for 10 minutes at room temperature and a wind speed of 3 to 6 m / s.
  • a support having seed crystals attached thereto was placed in a stainless steel pressure vessel having an internal volume of 300 ml, and the prepared raw material solution was placed. And the DDR type
  • the DDR type zeolite membrane was heated in an electric furnace (atmosphere, 450 ° C., 50 hours), and 11 adamantaneamine in the pores was burned and removed.
  • concentration of silica particles in the silica sol was 0.01% by mass.
  • the pH of the silica sol was adjusted to 8 by adding a few drops of hydrochloric acid (Aldrich) diluted with water to the silica sol.
  • the support was fixed to the lower end of the wide-mouth funnel, and 160 cc of silica sol was poured into each cell from above the support, thereby attaching the silica sol to the surface of the DDR type zeolite membrane.
  • the pH of the silica sol was set to 8
  • the support composed of alumina had a positive charge
  • the silica particles of the repair material had a negative charge
  • the membrane had a negative charge (see Figure 2). Therefore, the silica particles could be put into the defects of the DDR type zeolite membrane by attracting the silica particles to the support by Coulomb force.
  • Sample No. 4 was prepared except that a support was formed using mullite particles as an aggregate and the pH of the silica sol for the repair material was adjusted to 6. In the same process as in No. 1, sample no. A separation membrane structure according to No. 4 was produced.
  • Sample No. 5 Sample No. 4 was prepared except that a support was formed using mullite particles as an aggregate and the pH of silica sol, which is a colloid solution for repair material, was adjusted to 4. In the same process as in No. 1, sample no. A separation membrane structure according to No. 5 was produced.
  • a silica sol solution having an average particle diameter of 10 nm was diluted with water, and PVA as an organic binder was added to prepare a sol solution.
  • a silica UF (ultrafiltration) layer was formed on the inner surface of the cell by pouring the sol solution from above the support into each cell and passing it through the cell.
  • a mixed solution of metal alkoxide (titanium tetraisopropoxide) and nitric acid or hydrochloric acid is mixed with water while maintaining the temperature at 5 ° C., and further maintained at 25 ° C. and isopropyl alcohol or water previously mixed with nitric acid.
  • a sol stock solution was prepared by mixing with.
  • the titania sol-coating solution was obtained by diluting the sol stock solution with isopropyl alcohol (IPA) or water and adjusting to 0.1% by mass in terms of titania.
  • IPA isopropyl alcohol
  • the support was set in the film formation chamber, and the titania sol coating liquid was supplied from below the support at a liquid feed rate of 1.0 L / min using a liquid feed pump. Then, when excess sol liquid overflowed from above the support, the liquid feeding was stopped, and then the drain valve was opened to discharge the titania sol coating liquid.
  • the excess titania sol coating solution was removed by moving the support taken out from the film formation chamber so as to be shaken by hand. And it was made to dry for 10 hours using the air blower in the cell which discharged
  • the support was heated to 400 to 500 ° C. at 100 ° C./hr in an electric furnace, held for 1 hour, and then cooled at 100 ° C./hr to form a titania film on the silica UF layer.
  • titania sol was prepared by putting titania and ion-exchanged water in a container and stirring.
  • concentration of titania particles in the titania sol was 0.01% by mass.
  • the pH of the titania sol was adjusted to 6 by adding a few drops of hydrochloric acid diluted by water (made by Aldrich) to the titania sol.
  • the support was fixed to the lower end of the wide-mouth funnel, and 160 ml of titania sol was poured into each cell from above the support to attach the titania sol to the surface of the titania film.
  • the titania sol has a pH of 6
  • the support whose outermost layer is composed of silica has a negative charge
  • the titania particles of the repair material have a positive charge
  • the titania membrane as a separation membrane has a positive charge. (See FIG. 2).
  • the titania particles can be put into the defects of the titania film by attracting the titania particles to the support by Coulomb force.
  • Sample No. 9 Sample No. 4 was used except that alumina sol having a pH of 5 was used as the colloid solution for the repair material. In the same process as step 6, sample no. A separation membrane structure according to No. 9 was produced.
  • Sample No. 11 Sample No. 1 was used except that an alumina sol solution was used instead of the silica sol solution to form a UF layer on the cell inner surface of the support, and that a silica sol adjusted to pH 4 was used as the colloid solution for the repair material. In the same process as step 6, sample no. 11 was prepared.
  • the support composed of alumina has a positive charge
  • the silica particles of the repair material have a negative charge
  • the titania membrane as a separation membrane has a positive charge. It had a charge (see Figure 2).
  • Sample No. 12 Sample No. 1 was used except that a support was formed using zirconia particles as an aggregate, and silica sol adjusted to pH 4 was used as a colloid solution for a repair material. In the same process as step 6, sample no. A separation membrane structure according to No. 12 was produced.
  • the support composed of zirconia has a positive charge
  • the silica particles of the repair material have a negative charge
  • the titania membrane as a separation membrane has a positive charge. It had a charge (see Figure 2).
  • the separation factor was calculated from the equation ( 4 concentrations).
  • to calculate the CO 2 permeation amount by measuring the permeation flow rate of the gas passing through the DDR type zeolite membrane before defects repaired with a mass flow meter.
  • PEG aqueous solution was supplied to the titania membrane before defect repair, and the PEG blocking rate by the titania membrane was calculated from the PEG concentration ratio in the supply solution and the filtrate.
  • the absolute value of the zeta potential of the separation membrane does not exceed the absolute value of the zeta potential of the repair material particles.
  • the PEG blocking rate could be further increased. This is because the repairing material particles can be smoothly supplied to the defect by suppressing the repairing material particles from being repelled by the separation membrane by Coulomb force.
  • Sample No. The preparation steps 1-1 to 1-6 are the same as the sample Nos. Described above except that the concentration of the repair material particles in the colloid solution for repair is changed as shown in Table 3. Same as 1.
  • the separation factor was calculated from the equation ( 4 concentrations).
  • to calculate the CO 2 permeation amount by measuring the permeation flow rate of the gas passing through the DDR type zeolite membrane before defects repaired with a mass flow meter.
  • the separation factor could be increased by setting the concentration of the repair material particles in the colloidal solution to 0.01% by mass or more. This is because more repair material particles can be supplied to defects in the separation membrane by including a sufficient number of repair material particles in the colloid solution.
  • the decrease in the permeation amount could be suppressed by setting the concentration of the repair material particles in the colloid solution to 20% by mass or less. This is because the repair material particles can be prevented from adhering and remaining on the surface of the separation membrane by not including an excessive number of repair material particles in the colloidal solution.
  • the method for repairing a separation membrane according to the present invention is useful in the field of separation membranes because the separation performance of the separation membrane can be improved.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un procédé de réparation pour une membrane de séparation (30) comprenant une étape pour l'adhérence d'une solution colloïdale présentant un pH prédéterminé, des particules de matériau de réparation étant dispersées dans un solvant aqueux, à la surface de la membrane de séparation (30) formée sur un support (10). Au pH prédéterminé, les particules de matériau de réparation comprennent une charge électrique opposée à celle du support (10).
PCT/JP2016/081077 2015-11-18 2016-10-20 Procédé de réparation pour membrane de séparation et procédé de fabrication de structure de membrane de séparation WO2017086084A1 (fr)

Priority Applications (4)

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CN201680056179.XA CN108290123B (zh) 2015-11-18 2016-10-20 分离膜的修补方法和分离膜结构体的制造方法
JP2017551785A JP6767995B2 (ja) 2015-11-18 2016-10-20 分離膜の補修方法及び分離膜構造体の製造方法
DE112016005301.0T DE112016005301T5 (de) 2015-11-18 2016-10-20 Reparatur-Verfahren für eine Trennmembran und ein Verfahren zum Herstellen einer Trennmembranstruktur
US15/972,687 US11471836B2 (en) 2015-11-18 2018-05-07 Repair method for separation membrane and method for manufacturing separation membrane structure

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JP2015-225299 2015-11-18

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